Tetrahydrofuran → 4-(3-Chloro-1,4-dihydro-1,4-dioxo-2-naphthalenyl)-1-piperazinecarboxylic acid, 2-methylpropyl ester

HRID 622392

반응식

HRID 622392 반응식
[Cl:1][C:2]1[C:11](=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:13])[C:3]=1[N:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1.Cl[C:21]([O:23][CH2:24][CH2:25][CH2:26]C)=[O:22].O1CCC[CH2:29]1>>[Cl:1][C:2]1[C:11](=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:13])[C:3]=1[N:14]1[CH2:19][CH2:18][N:17]([C:21]([O:23][CH2:24][CH:25]([CH3:26])[CH3:29])=[O:22])[CH2:16][CH2:15]1

참가 물질

4

반응물 3

HCID 8028Tetrahydrofuran2회HCID 61140Butyl chloroformateHCID 6997941,4-Naphthalenedione, 2-chloro-3-(1-piperazinyl)-

생성물 1

HCID 139347664-(3-Chloro-1,4-dihydro-1,4-dioxo-2-naphthalenyl)-1-piperazinecarboxylic acid, 2-methylpropyl ester

실험 절차

A solution of 830 mg of 3-chloro-2-piperazinyl 1,4-naphthoquinone in 50 ml of tetrahydrofuran was added dropwise to a solution of 0.39 ml of butyl chloroformate in 10 ml of tetrahydrofuran. This mixture was stirred for 20 minutes, then filtered and the filtrate concentrated to an oil. The oil was crystallized from ether/hexane, giving 360 mg of the desired product, mp 92-94°C.

후처리

  1. filtrationfiltered
  2. concentrationthe filtrate concentrated to an oil
  3. customThe oil was crystallized from ether/hexane

출처 및 근거

ORD 기록
ord-787442818321466eb57083b50903aa55
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04771061

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